正相色谱串联质谱法直接进样测定水体中的草甘膦和2,4-滴残留  

Detection of Glyphosate and 2,4-D in Water by Normal-phase Chromatography Electrospray Ionization Tandem Mass Spectrometry

作　　者：郑和辉[1] 卞战强[1] 田向红[1] 于建[1] 查玉娥[1] 张娟[1] 

机构地区：[1]中国疾病预防控制中心农村改水技术指导中心

出　　处：《环境卫生学杂志》2014年第4期395-397,402,共4页JOURNAL OF ENVIRONMENTAL HYGIENE

基　　金：卫生行业科研专项(No.201302004)

摘　　要：目的建立直接进样测定饮用水和水源水中的草甘膦和2,4-滴的液相色谱质谱分析方法。方法采用正相色谱柱：CAPCELL PAK ST柱（2.1 mm×150 mm）,流动相为乙腈/10 mmol/L的乙酸铵水溶液（pH=10.10）。水样直接过0.22μm滤膜,用高效液相色谱串联质谱分析检测。结果草甘膦（100.0 ng/mL,400.0 ng/mL）和2,4-滴（10.0 ng/mL,40.0 ng/mL）在水中进行两个质量浓度的加标实验,每个质量浓度平行测定6次。通过测定和工作曲线的计算,得到草甘膦测定的结果为：95.3±3.8 ng/mL和402.7±20.8 ng/mL,即平均回收率分别为95.3%和100.7%;2,4-滴测定的结果为：9.7±0.2 ng/mL和38.6±1.0 ng/mL,即平均回收率分别为97.0%和96.5%。草甘膦在水中质量浓度范围在20.0-800.0 ng/mL,线性相关系数为0.9992;2,4-滴在水中质量浓度范围在2.0-80.0 ng/mL,线性相关系数为0.9996。在自来水中添加草甘膦和2,4-滴,以10倍信噪比（S/N）计算,在进样量10μL时;得到的本方法草甘膦和2,4-滴最低检测质量浓度分别为4.0 ng/mL和0.4 ng/mL。结论该方法简单,速度快,准确度和灵敏度高,满足测定日常地表水水体中百草甘膦和2,4-滴检测项目的需要。Objectives To setup a method for detecting glyphosate and 2,4-D in drinking water by liquid chromatography-tandem mass spectrometry（ LC-MS-MS）. Methods Using Chromatographic column： CAPCELL PAK ST（ 2. 1 mm × 150 mm） and mobile phase： acetonitrile /10 mmol /L ammonium acetate solution（ pH =10. 10） for the separation of samples; after passing a 0. 22 μm filter membrane,samples were detected by LC-MSMS. Results At spiked levels for glyphosate（ 100. 0 ng /mL,400. 0 ng /mL） in water,the detected concentrations were 95. 3 ± 3. 8 ng /mL and 402. 7 ± 20. 8 ng /mL,the average recoveries were 95. 3% and 100. 7%,and the linear regression coefficient for glyphosate at the concentration of 20. 0 ~ 800. 0 ng /mL was 0. 9992. At spiked levels for 2,4-D（ 10. 0 ng/mL,40. 0 ng/mL） in water,the detected concentrations were 9. 7 ± 0. 2 ng/mL and 38. 6 ±1. 0 ng/mL,the average recoveries were 97. 0% and 96. 5%,and the linear regression coefficient for 2,4-D at the concentration of 2. 0 ~ 80. 0 ng /mL was 0. 9996. The limit of detection（ S /N = 10） for glyphosate was 4. 0 ng /mL and for 2,4-D was 0. 4 ng /mL. Conclusions The method was simple and fast,had a good accuracy and high sensitivity,which could meet the needs for the determination of paraquat glyphosate and 2,4-D in drinking water.

关 键 词：草甘膦 2 4-滴 质谱 饮用水 正相色谱 

分 类 号：R123.1[医药卫生—环境卫生学] O657.63[医药卫生—公共卫生与预防医学]